US5454998A - Method for producing permanent magnet - Google Patents

Method for producing permanent magnet Download PDF

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Publication number
US5454998A
US5454998A US08/191,999 US19199994A US5454998A US 5454998 A US5454998 A US 5454998A US 19199994 A US19199994 A US 19199994A US 5454998 A US5454998 A US 5454998A
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United States
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sample
hydrogen
partial pressure
containing gas
hydrogen containing
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Expired - Fee Related
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US08/191,999
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English (en)
Inventor
Jacob G. Bogatin
Andrey Belov
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MNAP TECHNOLOGIES INTERNATIONAL Inc
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YBM Technologies Inc
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Assigned to YBM TECHNOLOGIES, INC. reassignment YBM TECHNOLOGIES, INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: BOGATIN, JACOB G., BELOV, ANDREY
Priority to US08/191,999 priority Critical patent/US5454998A/en
Priority to PCT/US1994/011526 priority patent/WO1995021452A1/en
Priority to EP95901683A priority patent/EP0696379A1/de
Priority to AU10823/95A priority patent/AU1082395A/en
Priority to CA002159463A priority patent/CA2159463A1/en
Priority to JP7520586A priority patent/JPH08508853A/ja
Priority to US08/437,719 priority patent/US5567891A/en
Publication of US5454998A publication Critical patent/US5454998A/en
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Assigned to MNAP TECHNOLOGIES INTERNATIONAL, INC. reassignment MNAP TECHNOLOGIES INTERNATIONAL, INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: YBM TECHNOLOGIES, INC.
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0573—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes obtained by reduction or by hydrogen decrepitation or embrittlement
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered

Definitions

  • This invention generally relates to magnetic materials and, more particularly, to rare earth element-containing powders and permanent magnets which contain hydrogen, and a process for producing the same.
  • Permanent magnet materials currently in use include alnico, hard ferrite and rare earth element-cobalt magnets. Recently, new magnetic materials have been introduced containing iron, various rare earth elements and boron. Such magnets have been prepared from melt quenched ribbons and also by the powder metallurgy technique of compacting and sintering, which was previously employed to produce samarium cobalt magnets.
  • U.S. Pat. No. 4,601,875 Yamamoto et al. teaches permanent magnet materials of the Fe--B--R type produced by: preparing a metallic powder having a mean particle size of 0.3-80 microns and a composition of, in atomic percent, 8-30% R representing at least one of the rare earth elements inclusive of Y, 2-28% B and the balance Fe; compacting: sintering at a temperature of 900°-1200° C.; and, thereafter, subjecting the sintered bodies to heat treatment at a temperature lying between the sintering temperature and 350° C.
  • Co and additional elements M may be present.
  • U.S. Pat. No. 4,802,931, Croat discloses an alloy with hard magnetic properties having the basic formula RE 1-x (TM 1-y B y ) x .
  • RE represents one or more rare earth elements including scandium and yttrium in Group IlIA of the periodic table and the elements from atomic number 57 (lanthanum) through 71 (lutetium).
  • TM in this formula represents a transition metal taken from the group consisting of iron or iron mixed with cobalt, or iron and small amounts of other metals such as nickel, chromium or manganese.
  • the Fruchart et al. patent teaches a new hydrogen containing alloy which contains H in an amount ranging from 0.1-5 atomic percent.
  • the alloy of Fruchart et al. is prepared by a process wherein the rare earth element-iron-boron compound at room temperature is hydrogenated under a hydrogen pressure above 10 bar (10 ⁇ 10 5 Pa) and below 500 bar (500 ⁇ 10 5 Pa). Following the hydrogenation process, the compound is subjected to a dehydrogenation cycle by subjecting it to temperatures ranging from 150° C. to 600° C., whereby all of the hydrogen is removed.
  • a permanent magnet of the type comprising a rare earth element-metal( e.g.,iron)-hydrogen-boron alloy which has high magnetic properties and elevated corrosion resistance. It is a further object of the invention to provide a process for preparing permanent magnets by treating a rare earth element-metal-boron material, such as an alloy, powder, green compact or permanent magnet material, in a hydrogen atmosphere at a temperature below the phase transformation temperatures of the rare earth element-metal hydrides, including temperatures below room temperature.
  • a rare earth element-metal-boron material such as an alloy, powder, green compact or permanent magnet material
  • a permanent magnet is provided which is comprised of, atomic percent: 10-24% R; 2-28% boron; 0.1-18.12% hydrogen; and balance being M.
  • R is at least one element selected from group consisting of: La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y and Sc
  • M is at least one metal selected from group consisting of: Fe, Co, Ni, Li, Be, Mg, As, Si, Ti, V, Cr, Mn, Cu, Zn, Ga Ge, Zn, Nb, Mo, Ru, Rh, Pd, Ag, Sb, Te, Hf, Ta, W, Re, Os, Ir, Pt, Au, and Bi.
  • the magnets produced according to the invention are permanent magnets containing from 0.1 to 18.12 atomic percent hydrogen and have high magnetic properties, e.g., residual induction (Br) up to 14.7 kG and maximum energy product (BHmax) up to 52.5 MGOe.
  • the permanent magnets according to this invention have elevated corrosion resistance.
  • one of the rare earth elements or a combination thereof, the metal and boron, as either the alloy, the powder form, green compact or as permanent magnet material, are first compacted, if that has not already been done.
  • the compacted sample is heated to at least the temperature necessary to achieve complete outgassing of the sample and is maintained in a high vacuum until outgassing is completed.
  • a partial pressure of hydrogen-containing gas is applied to the sample and the sample is heated in the hydrogen atmosphere to a temperature below the phase transformation temperature of the metal hydride and held at that temperature for the time necessary to saturate the sample with hydrogen and achieve the necessary atomic percent of hydrogen in the sample.
  • the hydrogen is replaced with argon, and the sample is thereafter heated again to the sintering temperature for the time necessary to achieve the required density of the magnet.
  • the resultant magnet is treated at 300° C. to 900° C. for approximately three hours in a partial pressure of argon, whereupon the formation and treatment process is completed.
  • this invention relates to permanent magnets of the rare earth element-metal-hydrogen-boron type. These magnets have been shown to have increased magnetic properties as well as increased corrosion resistance.
  • the permanent magnet is comprised of 10-24 atomic percent of at least one rare earth element; 2-28 atomic percent boron; 0.1-18.12 atomic percent hydrogen, with the remaining balance being at least one metal.
  • the rare earth element (R) includes at least one element selected from La Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y and Sc or a combination thereof.
  • the metal (M) includes at least one element selected from the group consisting of: Fe, Co, Ni, Li, Be, Mg, As, Si, Ti, V, Cr, Mn, Cu, Zn, Ga Ge, Zn, Nb, Mo, Ru, Rh, Pd, Ag, Sb, Te, Hf, Ta, W, Re, Os, Ir, Pt, Au, and Bi, and is preferably iron.
  • the introduction of a selected amount of hydrogen into the rare earth element-metal-boron crystal lattice forms a chemical composition of rare earth element and metal hydrides which results in the formation of the specific structure conditions in grain boundaries that lead to the nucleating and growth of the magnetic properties.
  • the availability of hydrogen diffused within the crystal lattice of the material makes it possible to reduce the number of impurities and their harmful effects, thus resulting in high corrosion resistance.
  • Permanent magnets comprising at least one of the rare earth elements, at least one metal, hydrogen and boron have levels of magnetic properties which would not exist without the inclusion of hydrogen.
  • the inclusion of hydrogen in the selected amounts disclosed herein has increased the level of magnetic properties, particularly the residual induction and maximum energy product, which have been shown to be as high as 14.7 kG and 52.5 MGOe, respectively.
  • the permanent magnets have shown increased corrosion resistance; for example, after treatment one of the permanent magnets prepared according to the present invention in 95% relative humidity for 500 hours at 85° C., the weight gain was less than 0.0008 g/cm 2 .
  • the permanent magnets according to the present invention also have been shown to have good workability or formability, which makes it possible to manufacture extremely small magnets in the range of 0.5 mm with good results. This must be compared with the usual workability of such magnets without the inclusion of the hydrogen component which are usually extremely brittle and difficult to shape into such small sizes. Magnets according to the present invention are far less brittle and are more easily shaped into these desired smaller sizes.
  • the compounds are prepared as follows.
  • the rare earth element or a combination thereof, the metal (or a combination thereof) and boron are first compacted, if that has not already been achieved.
  • the compacted sample is heated in a vacuum to the temperature necessary to obtain complete outgassing of the sample. In this instance, the sample is heated to 200° C. and held for 45 minutes in a vacuum at 10 -6 Torr.
  • a partial pressure of hydrogen containing gas is applied to the sample and the sample is heated in the hydrogen containing gas to a temperature below the phase transformation temperature of the metal hydride for the time necessary to saturate the sample with hydrogen, i.e., achieve the necessary atomic percent of hydrogen in the sample.
  • the magnetic properties of the resultant magnet can be varied with the atomic percent of hydrogen obtained in the sample as a result of varying the partial pressure of the hydrogen containing gas.
  • the hydrogen is replaced with argon (preferably 5"Hg) and the sample is heated to the sintering temperature for the time necessary to obtain the required density in the finished magnet product.
  • the sample is subjected to the argon at 5"Hg and sintered at 1090° C. for three more hours.
  • the resultant magnet is heat treated at temperatures between 300° C. and 900° C. for up to three hours in a partial pressure of argon.
  • the sintered magnet is treated at 900° C. for 1 hour and at 650° C. for two additional hours in a partial pressure of argon of 1"Hg.
  • the permanent magnet formation and treatment is complete.
  • the starting rare earth element-metal-boron powder contained, in weight percent: 31% Nd+3% Dy, 1.1% boron and the balance was iron.
  • the variable in each example is the parital pressure of hydrogen used to treat the compacted sample.
  • the process was conducted using a hydrogen containing gas having a partial pressure 4 ⁇ 10 -5 Torr.
  • the resulting hydrogen concentration in the magnets before exposure to air was 0.1 at % (atomic percent.)
  • the results of the treatment with hydrogen at a partial pressure of 4 ⁇ 10 -5 Torr are set forth in Table 1.
  • the average weight gain of the magnet after exposure to a relative humidity of 95% at 85° C. for 500 hours was 0.015 g/cm 2
  • the samples were subjected to a hydrogen containing gas having a partial pressure of 0.5 Torr.
  • the hydrogen concentration in the magnets of the second example, before exposure to air ranged from 0.41-0.54 at % (atomic percent).
  • the average weight gain after exposure to a relative humidity of 95% at 85° C. for 500 hours was 0.0009 g/cm 2 .
  • the samples were subjected to a hydrogen containing gas having a partial pressure of 0.75 Torr.
  • the hydrogen concentration on the magnets before exposure to air ranged from 0.78-0.88 at % (atomic percent).
  • the average weight gain after exposure to a relative humidity of 95% at 85° C. for 500 hours was 0.0011 g/cm 2 .
  • the samples were subjected to a hydrogen containing gas having a partial pressure of 1.1 Torr.
  • the hydrogen concentration on the magnets before exposure to air ranged from 1.20-1.29 at % (atomic percent).
  • the average weight gain after exposure to a relative humidity of 95% at 85° C. for 500 hours was 0.0025 g/cm 2 .
  • the samples were subjected to a hydrogen containing gas having a partial pressure of 1.5 Torr.As set forth in Table 5, the hydrogen concentration on the magnets before exposure to air ranged from 1.94-2.02 at % (atomic percent). Furthermore, the average weight gain after exposure to a relative humidity of 95% at 85° C. for 500 hours was 0.0032 g/cm 2 .
  • the samples were subjected to a hydrogen containing gas having a partial pressure of 5 Torr.
  • the hydrogen concentration on the magnets before exposure to air ranged from 17.98-18.12 at % (atomic percent).
  • the average weight gain after exposure to a relative humidity of 95% at 85° C. for 500 hours was 0.0051 g/cm 2 .
  • the increase in hydrogen in the rare earth element-metal-hydrogen-boron magnet material according to the process of the present invention results in increased magnetic properties and improved corrosion resistance.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Power Engineering (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Hard Magnetic Materials (AREA)
US08/191,999 1994-02-04 1994-02-04 Method for producing permanent magnet Expired - Fee Related US5454998A (en)

Priority Applications (7)

Application Number Priority Date Filing Date Title
US08/191,999 US5454998A (en) 1994-02-04 1994-02-04 Method for producing permanent magnet
CA002159463A CA2159463A1 (en) 1994-02-04 1994-10-11 Rare earth element-metal-hydrogen-boron permanent magnet and method of production
EP95901683A EP0696379A1 (de) 1994-02-04 1994-10-11 Dauermagnet aus seltenerdmetall,wasserstoff und bor und sein herstellungsverfahren
AU10823/95A AU1082395A (en) 1994-02-04 1994-10-11 Rare earth element-metal-hydrogen-boron permanent magnet and method of production
PCT/US1994/011526 WO1995021452A1 (en) 1994-02-04 1994-10-11 Rare earth element-metal-hydrogen-boron permanent magnet and method of production
JP7520586A JPH08508853A (ja) 1994-02-04 1994-10-11 希土類元素−金属−水素−ホウ素永久磁石およびその製造方法
US08/437,719 US5567891A (en) 1994-02-04 1995-05-08 Rare earth element-metal-hydrogen-boron permanent magnet

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US08/191,999 US5454998A (en) 1994-02-04 1994-02-04 Method for producing permanent magnet

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US08/437,719 Continuation US5567891A (en) 1994-02-04 1995-05-08 Rare earth element-metal-hydrogen-boron permanent magnet

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US08/437,719 Expired - Fee Related US5567891A (en) 1994-02-04 1995-05-08 Rare earth element-metal-hydrogen-boron permanent magnet

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EP (1) EP0696379A1 (de)
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AU (1) AU1082395A (de)
CA (1) CA2159463A1 (de)
WO (1) WO1995021452A1 (de)

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US20030047240A1 (en) * 2000-09-20 2003-03-13 Aichi Steel Corporation Manufacturing method of an anisotropic magnet powder, precursory anisotropic magnet powder and bonded magnet
US20040250799A1 (en) * 2003-06-13 2004-12-16 Wout Lisseveld Fuel treatment device using a magnetic field
US20070181219A1 (en) * 2004-08-23 2007-08-09 Nissan Motor Co., Ltd. Alloy thin ribbon for rare earth magnet, production method of the same, and alloy for rare earth magnet
WO2009116867A2 (en) * 2008-03-21 2009-09-24 Asml Netherlands B.V. A target material, a source, an euv lithographic apparatus and a device manufacturing method using the same
CN1901105B (zh) * 2005-07-18 2010-05-12 漯河市三鑫稀土永磁材料有限责任公司 高耐温性hddr钕铁硼各向异性磁粉
CN103632790A (zh) * 2013-12-19 2014-03-12 江苏南方永磁科技有限公司 一种高磁能积钕铁硼永磁材料及其制备方法
US9044834B2 (en) 2013-06-17 2015-06-02 Urban Mining Technology Company Magnet recycling to create Nd—Fe—B magnets with improved or restored magnetic performance
US9336932B1 (en) 2014-08-15 2016-05-10 Urban Mining Company Grain boundary engineering

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US6332933B1 (en) 1997-10-22 2001-12-25 Santoku Corporation Iron-rare earth-boron-refractory metal magnetic nanocomposites
CN1265401C (zh) 1998-07-13 2006-07-19 株式会社三德 制造纳米复合磁性材料的方法以及制造粘结磁体的方法
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CN1142560C (zh) * 1999-09-14 2004-03-17 北京大学 多元间隙型永磁材料及其磁粉、磁体的制造工艺
US6136100A (en) * 1999-09-29 2000-10-24 Magnequench International, Inc. Rare-earth alloy powders for magnets and process for making magnets from rare-earth alloy powders
US8821650B2 (en) * 2009-08-04 2014-09-02 The Boeing Company Mechanical improvement of rare earth permanent magnets
CN103106992B (zh) * 2013-02-06 2015-05-13 江苏南方永磁科技有限公司 一种高弯曲抗力永磁材料及制备方法
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CN1901105B (zh) * 2005-07-18 2010-05-12 漯河市三鑫稀土永磁材料有限责任公司 高耐温性hddr钕铁硼各向异性磁粉
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US9044834B2 (en) 2013-06-17 2015-06-02 Urban Mining Technology Company Magnet recycling to create Nd—Fe—B magnets with improved or restored magnetic performance
US9067284B2 (en) 2013-06-17 2015-06-30 Urban Mining Technology Company, Llc Magnet recycling to create Nd—Fe—B magnets with improved or restored magnetic performance
US9095940B2 (en) 2013-06-17 2015-08-04 Miha Zakotnik Harvesting apparatus for magnet recycling
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CN103632790B (zh) * 2013-12-19 2016-06-01 江苏南方永磁科技有限公司 一种高磁能积钕铁硼永磁材料及其制备方法
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WO1995021452A1 (en) 1995-08-10
JPH08508853A (ja) 1996-09-17

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